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US20140199738A1 - Method for preparing volatile fatty acids from the pre-treated extracts of marine biomass residue - Google Patents

Method for preparing volatile fatty acids from the pre-treated extracts of marine biomass residue Download PDF

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US20140199738A1
US20140199738A1 US13/807,587 US201113807587A US2014199738A1 US 20140199738 A1 US20140199738 A1 US 20140199738A1 US 201113807587 A US201113807587 A US 201113807587A US 2014199738 A1 US2014199738 A1 US 2014199738A1
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algae
acid
vfas
extract
residue
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Hee-chul Woo
Ho-Nam Chang
Yeong-Joong Jeon
Dong-Jin Suh
Byung-Soo Chun
Kyeong-Keun Oh
Kyoung-Heon Kim
Du-Woon Kim
Jae-Hyung Choi
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Pukyong National University
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Pukyong National University
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
    • C12P7/6409—Fatty acids
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
    • C12N1/20—Bacteria; Culture media therefor
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
    • C12P7/52—Propionic acid; Butyric acids
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
    • C12P7/54—Acetic acid
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Definitions

  • Example embodiments of the present invention relate in general to a method of preparing a volatile fatty acid, and more particularly, to a method of preparing a volatile fatty acid using a residue of algae (marine algae biomass) that remains after extracting or fractionating the algae with an organic solvent.
  • Biofuel refers to a fuel obtained from a biomass. Such biofuel can be produced by subjecting a biomass to a thermochemical or biological method. A variety of biofuels can be produced using such a method.
  • an anaerobic fermentation platform or a volatile fatty acid (VFA) platform
  • VFA volatile fatty acid
  • an anaerobic fermentation platform is a method that includes mixing biomass with an anaerobic microorganism and incubating the anaerobic microorganism to degrade the biomass into a VFA mixture and optionally converting the VFA mixture into a gaseous fuel such as hydrogen to recover the gaseous fuel or converting the VFA mixture into a liquid fuel including an alcohol mixture using a hydrogenation reaction.
  • VFAs produced by such a VFA platform is composed of acetic acid (C2), propionic acid (C3), butyric acid (C4), etc., which are then converted into ethanol, propanol, butanol, etc., respectively, through the hydrogenation reaction.
  • C2 acetic acid
  • C3 propionic acid
  • C4 butyric acid
  • the MixAlco technology developed at Texas A&M University (US) is a representative method of producing a mixed alcohol from wood using the described-above VFA platform, and is now in final case study.
  • Biomasses are largely divided into three categories: first generation (sugar or starch biomasses), second generation (lignocellulosic biomass) and third generation (marine algae biomass). Each biomass can undergo a pretreatment process and a saccharification process, followed by a fermentation process to produce a biofuel.
  • first generation sucrose or starch biomasses
  • second generation lignocellulosic biomass
  • third generation marine algae biomass.
  • Each biomass can undergo a pretreatment process and a saccharification process, followed by a fermentation process to produce a biofuel.
  • the biomasses other than the lignocellulosic biomasses that is, the sugar or starch biomasses
  • the biomasses other than the lignocellulosic biomasses that is, the sugar or starch biomasses
  • foods that should be used as an energy source are ineffective because the biofuel is produced at a relatively smaller amount than that of the biomass being consumed.
  • the lignocellulosic biomass have a problem in that economical efficiency is lowered due to the additional processing costs required for a pretreatment process to remove lignin that is a component of lignocellulosic biomass.
  • such terrestrial biomasses have a problem in that environmental issues may be caused due to the use of fertilizers.
  • the soil is insufficient for producing the land biomasses.
  • a VFA platform using such an algae biomass has advantages in that it can convert organic components (proteins, lipids, etc.) other than carbohydrates into VFAs, does not require a sterilization process to incubate a strain, and there is no need to develop a certain enzyme. Also, it is known that, since the most of algae biomass does not include a lignin component, it takes a short period of time (e.g., from five to ten days) to produce VFAs. In addition, an enclosed reactor can be used to recover hydrogen produced during fermentation of a VFA, the recovered hydrogen can be easily used for a subsequent hydrogenation reaction, and it is easy to handle problems regarding a bad smell which is expected to be a problem of the VFA platform.
  • example embodiments of the present invention are provided to substantially obviate one or more problems due to limitations and disadvantages of the related art.
  • Example embodiments of the present invention provide a method of producing volatile fatty acids (VFAs) with high efficiency using a filtrate of an extract obtained by pretreating and extracting a residue of an algae biomass extract or fraction.
  • VFAs volatile fatty acids
  • a method of preparing VFAs includes collecting a residue of algae that remains after extracting or fractionating the algae with an organic solvent, chemically or biologically pretreating the residue of algae to obtain an extract of the algae residue, filtering the extract of the algae residue to obtain a filtrate and anaerobically fermenting the filtrate.
  • FIG. 1 is a flowchart schematically showing a method of preparing volatile fatty acids (VFAs) according to Example embodiments of the present invention.
  • FIG. 2 is a diagram showing a fermentation apparatus used for anaerobic fermentation according to Example embodiments of the present invention.
  • FIG. 3 is a graph showing the compositions of VFAs according to kinds of algae.
  • FIG. 4 is a graph showing the compositions of VFAs according to pretreatment conditions 1 to 4 described in Example ⁇ 2-3> of the present invention.
  • FIG. 5 is a graph showing the compositions of VFAs according to pretreatment conditions 5 to 8 described in Example ⁇ 2-3> of the present invention.
  • FIG. 6 is a graph showing the compositions of VFAs according to pretreatment conditions 9 to 12 described in Example ⁇ 2-3> of the present invention.
  • FIG. 7 is a graph showing the compositions of VFAs according to a change in anaerobic fermentation temperature.
  • FIG. 8 is a graph showing the compositions of VFAs according to a change in anaerobic fermentation acidity.
  • FIG. 9 is a graph showing the compositions of VFAs according to the kinds of methane production inhibitors added during anaerobic fermentation.
  • FIG. 10 is a graph showing the compositions of VFAs according to the kinds of medium compositions (medium 1 to medium 3) in which an anaerobic microorganism is incubated during anaerobic fermentation.
  • FIG. 11 is a graph showing the compositions of VFAs according to the kinds of medium compositions (media 4 and 5) in which an anaerobic microorganism is incubated during anaerobic fermentation.
  • FIG. 12 is a diagram showing a 300 L continuous anaerobic fermentation apparatus.
  • Example embodiments of the present invention are disclosed herein. However, specific structural and functional details disclosed herein are merely representative for purposes of describing example embodiments of the present invention, however, example embodiments of the present invention may be embodied in many alternate forms and should not be construed as limited to example embodiments of the present invention set forth herein.
  • Example embodiments of the present invention provide a method of preparing a volatile fatty acid (VFA) including: 1) collecting a residue of algae biomass that remains after extracting or fractionating the algae with an organic solvent, 2) chemically or biologically pretreating the residue of algae to obtain an extract of the algae residue, 3) filtering the extract of the algae residue to obtain a filtrate, and 4) anaerobically fermenting the filtrate.
  • VFA volatile fatty acid
  • Step 1) is to collect a dreg, for example, a residue of an algae extract or fraction, which remains after extracting or fractionating algae with an organic solvent, followed by extracting or fractionating soluble materials included in the algae.
  • the method of preparing a VFA according to Example embodiments of the present invention does not use an extract or fraction obtained by primarily extracting or fractionating algae, but re-uses a waste material such as a dreg (residue) that remains after extracting or fractionating the algae so as to produce VFAs.
  • the algae in Step 1) may be macro-algae or micro-algae.
  • the macro-algae may include brown algae, red algae or green algae, and the micro-algae may include Chlorella, Spirulina or Dunaliella sp.
  • the brown algae may include, but is not limited to, Laminaria japonica, Undaria pinnatifida, Hizikia fusiforme, Sargassum fulvellum, Ecklonia stolonifera, Analipus japonicus, Chordaria flagelliformis, Ishige okamurae, Scytosiphon lomentaria, Endarachne binghamiae, Ecklonia cava, Costaria costata, Sargassum horneri, Sargassum thunbergii or Eisenia bicyclis .
  • the red algae may include, but is not limited to, Pachymeniopsis elliptica, Porphyra umbilicalis, Gelidium amansii, Cottonni, Pachymeniopsis lanceolata, Pachymeniopsis suborbiculata, Pterocladia tenuis, Acanthopeltis japonica, Gloiopeltis tenax, Chondrus ocellatus, Grateloupia elliptica, Hypnea sp., Ceramium sp., Ceramium boydenii, Chondracanthus tenellus, Graptoloidea sp., Pachymeniopsis elliptica or Gracilaria verrucosa
  • the green algae may include, but is not limited to, Sphagnum sp., Spirogyra sp., Ulva pertusa, Codium fragile, Codium minus, Caulerpa sp., Nostoc s
  • the algae of Step 1) may be physically pretreated to enhance pretreatment efficiency by enlarging a reaction surface area during extraction or fractionation of algae.
  • the physical pretreatment means that algae are ground or cut, and may be performed using all kinds of tools capable of grinding or cutting the algae. Especially, the physical pretreatment may be performed using a ball mill or a knife.
  • the residue of algae obtained in Step 1) is a dreg remaining after extraction or fractionation with the organic solvent, that is, a dreg of algae remaining after directly dissolving or separating soluble materials (i.e., materials soluble in an organic solvent) from algae directly or through respective operations and extracting or fractionating the soluble materials included in the algae.
  • the organic solvent that may be used herein may include at least one selected from the group consisting of ethanol, n-hexane, dichloromethane, ethylacetate and n-butanol.
  • Steps 2) to 4) are to produce VFAs using the dreg remaining after extracting or fractionating the soluble materials in the organic solvent in Step 1).
  • the term “residue of algae” or “algae residue” used herein refers to a “dreg remaining after primarily extracting or fractionating the algae obtained in Step 1) using an organic solvent.”
  • Step 2) is to pretreat the residue of algae so as to produce VFAs from the residue of algae obtained in Step 1).
  • the residue of algae may be chemically or biologically pretreated.
  • materials used to produce the VFAs from the algae residue are extracted, thereby obtaining an extract of the algae residue.
  • the chemical pretreatment of Step 2) may be performed by treating the algae residue with at least one selected from the group consisting of an acid catalyst, an alkali catalyst and a supercritical fluid.
  • the acid catalyst may be at least one selected from the group consisting of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, perchloric acid, p-toluenesulfonic acid, methanesulfonic acid, formic acid, acetic acid, hydrofluoric acid, boric acid and a commercially available solid acid
  • the alkali catalyst may be at least one selected from the group consisting of potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, ammonium hydroxide and basic zeolite
  • the supercritical fluid may be supercritical carbon dioxide or supercritical water.
  • the pretreatment with the acid catalyst may be performed using a first acid catalyst treatment method in which a reaction is carried out in a batch-type reactor and a second acid catalyst treatment method in which a reaction is carried out in a reflux-type reactor. According to Example embodiments of the present invention, it is confirmed that the pretreatment using the first acid catalyst treatment method in which a reaction is carried out in a batch-type reactor is more effective in producing VFAs.
  • the biological pretreatment of Step 2) may be performed by treating the algae residue with a culture broth including a microorganism.
  • the microorganism may be derived from abalone viscera or foreshore.
  • the abalone viscera- or foreshore-derived microorganism shows halophilicity and has a characteristic of easily taking in and digesting the algae.
  • the filtration of Step 3) is to obtain an extract extracted from the algae residue, that is, only a liquid including materials that are derived from the algae residue and used to produce the VFAs.
  • the filtrate obtained by the filtration may be used to produce the VFAs. That is, a solid product of the pretreated algae residue is not used, but a filtrate obtained by filtering the extract derived from the algae residue is used herein.
  • the extract of the algae residue is a mixture including a carbohydrate such as a fermentable sugar (glucose, fucose, mannitol, etc.), a non-degradable sugar (alginate, uronic acid, etc.), a protein, a lipid and a compound whose molecular weight is reduced by the pretreatment as main components.
  • the components constituting the extract of the algae residue described above may be used as a carbon source to produce the VFAs.
  • the solid product of the pretreated algae may be separately separated without use for production of VFAs, and may be used as a raw material such as a composite biomaterial, a natural fertilizer or bio-oil, which is used for a fast pyrolysis process.
  • Example embodiments of the present invention only volatile organic acids are not produced using the total solid algae as a raw source like technologies known in the art, but VFAs are produced from a residue of algae remaining after primary recovery (extraction or separation) of physiologically active materials from the algae and the pretreated solid product is used as a raw material such as a composite biomaterial, a natural fertilizer or bio-oil so that the use of an algae source can be maximized and the economical efficiency can be secured.
  • the filtrate of Step 4) preferably has a concentration of 6 g/L to 84 g/L, and more preferably a concentration of 18 g/L to 54 g/L.
  • concentration of the filtrate is less than 6 g/L, it takes more expense to recover the produced VFAs due to their low concentration.
  • concentration of the filtrate exceeds 84 g/L, a concentration of the produced VFAs is not increased any more, and thus the yield of the VFAs may be decreased with an increase in amount of an unreacted extract.
  • the concentration of the filtrate from the extract of the algae residue may be adjusted to this concentration range by diluting or concentrating the filtrate from the extract of the algae residue. According to Example embodiments of the present invention, it is confirmed that the VFAs may be most effectively produced when the extract filtrate is present within this concentration range.
  • the anaerobic fermentation of Step 4) may be performed using an anaerobic microorganism.
  • the filtrate obtained in Step 3) is fermented with an anaerobic microorganism, the filtrate is fermented under the anaerobic condition.
  • the anaerobic microorganism may be an anaerobic fermentation strain widely used in the art. Here, the use of an anaerobic fermentation strain having salt tolerance is preferred.
  • the anaerobic fermentation strain may be isolated from the viscera or excretion of an herbivorous animal such as a cow or a goat, an acid fermentation tank for methane production, a methane fermentation tank, an anaerobic fermentation tank for food waste, and a site (such as foreshore) having a high activity of degrading organic matters.
  • the anaerobic fermentation strain may be at least one selected from the group consisting of Clostridium sp., Acetogenium sp., Peptococcus sp., Acetobacterium sp., Pseudomonas sp. and Propionobacterium sp.
  • the anaerobic microorganism may be introduced at a volume ratio of 1/30 to 1/10, based on the volume of the filtrate to be fermented.
  • a volume ratio of 1/30 it takes more expense to recover the produced VFAs due to their low concentration.
  • the amount of the introduced anaerobic microorganism exceeds a volume ratio of 1/10, a concentration of the produced VFAs is not increased any more, and thus the yield of the VFAs may be decreased with an increase in amount of an unreacted extract.
  • it is confirmed that production of the VFAs is most effective when the anaerobic microorganism is introduced at a volume ratio of 1/15.
  • the anaerobic fermentation of Step 4) may be performed in the presence of a methane production inhibitor.
  • the methane production inhibitor functions to prevent a decrease in concentration of the VFAs by preventing the VFAs from being converted into methane by a methane-producing microorganism in an anaerobic fermentation process.
  • the methane production inhibitor may further improve production efficiency of the volatile organic acids.
  • CHI 3 or CHBr 3 may be used as the methane production inhibitor.
  • it is confirmed that production of the VFAs is the most effective when CHI 3 is used as the methane production inhibitor.
  • the anaerobic fermentation of Step 4) plays an important role in regulating pH and osmotic pressure, and may be performed in a medium including a microorganism and an inorganic salt.
  • the inorganic salt may be at least one selected from the group consisting of inorganic salts such as ammonium salt, phosphate, calcium salt, magnesium salt and sodium salt.
  • the medium may include (NH 2 ) 2 CO as a nitrogen source and KH 2 PO 4 as a phosphorus source. According to Example embodiments of the present invention, it is confirmed that it is most effective to produce the VFAs in a medium including (NH 2 ) 2 CO and KH 2 PO 4 so that nitrogen and phosphorus can be present at a molar ratio of 1.5:1 to 7.5:1.
  • the VFAs produced through the anaerobic fermentation may include, but are not limited to, propionic acid, butyric acid, valeric acid or caproic acid, as well as acetic acid (i.e., both of the iso- and normal formation).
  • kinds of the produced VFAs may vary according to the conditions such as fermentation acidity (pH), fermentation temperature, kinds of algae, etc.
  • PH fermentation acidity
  • a person skilled in the art can selectively produce a desired VFA by properly adjusting the conditions.
  • Example ⁇ 1-1> The residue of algae obtained in Example ⁇ 1-1> was chemically or biologically pretreated using methods listed in the following Table 1, and the alga pretreated as described above was filtered to obtain a filtrate.
  • Concentrations of the extract filtrates are listed in the following Table 2.
  • the concentrations listed in the following Table 2 were calculated according to the following Equation 1.
  • a concentration of the extract filtrate was adjusted to a desired level by diluting or concentrating the extract filtrate.
  • Pretreatment type Pretreatment method Condition Biological Microorganism Kind of microorganism: abalone viscera-derived pretreatment treatment method microorganism kind of culture broth: LB broth (tryptone, yeast extract, sodium chloride) Culture temperature and time: 37° C., 36 hours
  • Chemical First acid catalyst Reaction system batch-type autoclave reactor pretreatment treatment method
  • Catalyst An aqueous solution containing 3 wt % H 2 SO 4 Reaction time: 250 minutes
  • Second acid catalyst Reaction system reflux-type autoclave reactor treatment method
  • Catalyst An aqueous solution containing 5 wt % H 2 SO 4 Reaction time: 500 minutes
  • Base catalyst treatment Reaction system batch-type autoclave reactor method
  • Catalyst An aqueous solution containing 1 wt % NaOH Reaction temperature: 120° C.
  • Step 1 Treatment with supercritical carbon dioxide> treatment method after Reaction system: continuous autoclave extraction treatment with apparatus supercritical carbon Catalyst and solvent: carbon dioxide dioxide Reaction temperature and pressure: 45° C., 200 bars Reaction time: 1 hour
  • Step 2 Treatment with supercritical carbon dioxide>
  • Treatment with Reaction system batch-type autoclave reactor supercritical water Catalyst and solvent: water Reaction temperature and pressure: 300° C., 250 bars Reaction time: 1 minute
  • Example ⁇ 1-2> The filtrate obtained in Example ⁇ 1-2> was diluted, and a medium having a composition listed in the following Table 3 and a methane production inhibitor were put into a fermentation apparatus shown in FIG. 2 together with a microorganism (at a volume ratio of 1/15, that is, 0.06 L of a microorganism based on a 0.9 L of a fermentation solution) (obtained from an anaerobic fermentation tank in a sewage disposal plant at SuYoung, Busan). Thereafter, nitrogen gas was added for 10 minutes so as to remove oxygen gas in the fermentation apparatus.
  • a microorganism at a volume ratio of 1/15, that is, 0.06 L of a microorganism based on a 0.9 L of a fermentation solution
  • the pH value was maintained to a desired constant level by adding a 3 M NH 4 HCO 3 solution when the pH value decreased and a 3 M H 2 PO 4 solution when the pH value increased. Also, a fermentation temperature in the fermentation apparatus was maintained to a desired constant level using a thermostat. Nitrogen gas was added from the bottom of the fermentation apparatus to mix the components in the fermentation apparatus, and the mixing was performed twice a day. The yield of VFAs from the collected samples was quantified using a gas chromatography with flame ionization detector (Shimadzu 17A), and calculated according to the following Equation 2.
  • VFAs were produced from a residue of an algae extract in the same manner as in Example 1, except that the conditions such as a pretreatment method, kinds of algae, a concentration of an extract, a volume ratio of a microorganism, a fermentation temperature and fermentation pH were changed to analyze the concentration and yield of the VFAs.
  • the VFAs were produced while constantly maintaining all the other conditions listed in the following Tables 4 to 6, except for the pretreatment method performed before anaerobic fermentation.
  • the algae extracts pretreated using a first acid catalyst treatment method, a base catalyst treatment method and a supercritical water treatment method were compared with each other. As a result, it could be seen that the highest concentration and yield of the VFAs were produced from the residue of the algae extract pretreated using the first acid catalyst treatment method and the base catalyst treatment method, as listed in Table 4.
  • the algae extracts pretreated using a first acid catalyst treatment method and a microorganism treatment method were compared with each other.
  • a concentration of the Laminaria japonica extract was 54 g/L as listed in Table 4, which was relatively higher than a concentration (6 g/L) of the extract obtained when Laminaria japonica was pretreated using the microorganism treatment method.
  • the Laminaria japonica extract was properly diluted to a concentration of 6 g/L for comparison with the microorganism treatment method.
  • the VFAs were produced with relatively higher concentration and yield in the microorganism treatment method than in the first acid catalyst treatment method, as listed in Table 5. From the described-above results, it could be seen that, when the extract was obtained from the algae residue using the microorganism treatment method, a large amount of the components from which the VFAs were produced was selectively included in the extract.
  • the algae extracts pretreated using a first acid catalyst treatment method, a second acid catalyst treatment method and a supercritical water treatment method were compared with each other.
  • the VFAs were produced with the highest concentration and yield from the algae extract pretreated using the first acid catalyst treatment method, as listed in Table 6.
  • the second acid catalyst treatment method might be advantageous for mass production due to low apparatus costs since it does not require a high-pressure reactor, compared with the first acid catalyst treatment method.
  • the VFAs were produced with high concentration and yield from the algae extracts pretreated using the first acid catalyst treatment method and the base treatment method. Among these, it could be seen that the first acid catalyst treatment method was most effective. Therefore, in the following experiments using the other conditions, the algae were pretreated using the first acid catalyst treatment method, and the concentration and yield of the VFAs were compared and analyzed.
  • the VFAs were produced while constantly maintaining all the other conditions listed in the following Table 7, except that the different kinds of the algae, for example, Laminaria japonica, Pachymeniopsis lanceolata, Enteromorpha crinita and Chlorella , were used, and the different pretreatment methods, for examples, a first acid catalyst treatment method, a second acid catalyst treatment method and a base catalyst treatment method, were used herein.
  • the different kinds of the algae for example, Laminaria japonica, Pachymeniopsis lanceolata, Enteromorpha crinita and Chlorella
  • the different pretreatment methods for examples, a first acid catalyst treatment method, a second acid catalyst treatment method and a base catalyst treatment method, were used herein.
  • the VFAs were produced with high concentration and yield from all kinds of the algae regardless of the pretreatment method, as listed in Table 7.
  • the compositions of the produced VFAs varied according to the kinds of the algae, as shown in FIG. 3 .
  • a relatively high concentration of acetic acid was produced from the brown algae, Laminaria japonica , and the green algae, Enteromorpha crinita , and acetic acid, propionic acid and butyric acid were produced in order of increasing concentration from the red algae, Pachymeniopsis lanceolata.
  • the VFAs were produced while constantly maintaining all the other conditions listed in the following Table 8, except that the pretreatment conditions for the first acid catalyst treatment method, for example, a reaction temperature, an acid catalyst concentration and a reaction time, were changed.
  • the VFAs were readily produced under the pretreatment conditions such as a reaction temperature of 100° C. to 120° C., an acid catalyst concentration of 1 wt % to 10 wt % and a reaction time of 100 to 400 minutes, and reached the maximum concentration 5 days after the anaerobic fermentation, as listed in Table 8.
  • the compositions of the produced VFAs were different according to the pretreatment conditions, as shown in FIG. 4 to FIG. 6 .
  • acetic acid, propionic acid and butyric acid were produced in order of increasing concentration
  • butyric acid, caproic acid and valeric acid were produced in an increasing concentration as the reaction time progressed.
  • the VFAs were produced while constantly maintaining all the other conditions listed in the following Table 9, except that the pretreated algae extract was used at different concentrations of 18 g/L, 36 g/L, 54 g/L and 72 g/L.
  • a concentration of the VFAs was increased with an increasing concentration of the extract of the pretreated algae residue, and the concentration of the VFAs was not increased when the extract was present at a concentration of 54 g/L or more, as listed in Table 9. This indicates that a microorganism reached its limit to produce the VFAs, and thus the concentration of the VFAs was not increased any more, and the yield of the VFAs was decreased due to an increase of an unreacted extract.
  • VFAs were produced while constantly maintaining all the other conditions listed in the following Table 10, except that an extract of the Laminaria japonica residue pretreated using a first acid catalyst treatment method, a supercritical water treatment method after treatment with supercritical carbon dioxide and a supercritical water treatment method was treated with an anaerobic fermentation microorganism at volume ratios of 1/30, 1/15 and 1/10, based on the total amount of the filtrated to be fermented, to produce VFAs.
  • the concentration and yield of the VFAs increased with an increasing volume ratio of the microorganism regardless of the pretreatment method, and the microorganism was used at the optimum volume ratio of 1/15, as listed in Table 10.
  • the microorganism was used at a volume ratio of 1/15 or more, a concentration of the produced VFAs was not increased any more, and an amount of microorganism sludge increased, which leads to an increase in separation costs.
  • VFAs were produced while constantly maintaining all the other conditions listed in the following Table 11, except for different fermentation temperatures of 25° C., 35° C. and 45° C.
  • the produced VFAs were produced at the highest concentration and yield, as listed in Table 11 and shown in FIG. 7 . Also, for the compositions of the produced VFAs, acetic acid and propionic acid were produced at relatively high concentrations at 25° C., acetic acid was produced at a relatively high concentration at 35° C., and acetic acid and butyric acid were produced at relatively high concentrations at 45° C.
  • VFAs were produced while constantly maintaining all the other conditions listed in the following Table 12, except for different fermentation acidities of pH 6, pH 6.5 and pH 7.
  • the concentration and yield of the VFAs increased according to a reaction time regardless of the fermentation acidity, and, for the compositions of the produced VFAs, acetic acid, propionic acid and butyric acid were produced at similar concentrations at pH 6, acetic acid and propionic acid were produced at relatively high concentrations at pH 6.5, and acetic acid was produced at a relatively high concentration at pH 7, as listed in Table 12 and shown in FIG. 8 .
  • VFAs were produced while constantly maintaining all the other conditions listed in the following Table 13, except that a methane production inhibitor was not added, or different kinds of the added methane production inhibitor such as CHI 3 and CHBr 3 were used.
  • the VFA was produced at relatively high speed for 5 days when there was no methane production inhibitor, and there was no significant difference in concentration of the VFAs after 10 days, as listed in Table 13.
  • acetic acid was produced at a relatively high concentration when the methane production inhibitor was not used
  • acetic acid and butyric acid were produced at relatively high concentrations when CHBr 3 was used
  • acetic acid and propionic acid were produced at relatively high concentrations at the beginning when CHI 3 was used.
  • the methane production inhibitor functions to prevent a reduction in concentration of the VFAs by preventing the VFAs from being converted into methane by a methane-producing microorganism during an anaerobic fermentation process.
  • a microorganism was added at a volume ratio of 1/15 to 18 g/L of the extract of the pretreated algae obtained by the second acid catalyst treatment method, and anaerobically fermented at conditions of 35° C. and pH 7 in a fermentation medium including N and P at a molar ratio of 3.5:1 to produce VFAs, except that compositions of the fermentation medium varied as listed in the following Table 14.
  • a microorganism and CHI 3 (a methane production inhibitor) were added at a volume ratio of 1/15 to 18 g/L of the extract of the pretreated algae obtained by the second acid catalyst treatment method, and anaerobically fermented at conditions of 35° C. and pH 7 in a medium containing (NH 2 ) 2 CO and KH 2 PO 4 to produce VFAs, except that the N:P molar ratios in the fermentation media varied as listed in the following Table 15.
  • the method of preparing a VFA according to Example embodiments of the present invention can be useful in using a residue of an algae extract or fraction from which physiologically active materials are primarily recovered. Therefore, it is possible to enhance added value of the residue of the wasted algae, which makes it possible to secure the economical efficiency in production of biofuel or compounds.
  • the VFAs can be produced regardless of the kinds of algae, and a process of producing a VFA can be simplified since there is no need to develop an enzyme for anaerobic fermentation.
  • the VFAs can be produced from the other kinds of organic components such as proteins or fats, which constitute the algae, in addition to carbohydrates included in the algae, it is possible to enhance the yield of the VFAs.
  • the method according to Example embodiments of the present invention can be useful in producing VFAs in an economical and efficient manner.

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CN117210512A (zh) * 2023-09-27 2023-12-12 东华大学 等离子体耦合离子液体促进污泥产短链脂肪酸的应用
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US11891455B2 (en) 2019-09-23 2024-02-06 Galimedix Therapeutics Inc Polymorph form of (r)-2-[2-amino-3-(indol-3-yl)propionylamino]-2- methylpropionic acid and uses thereof
CN117210512A (zh) * 2023-09-27 2023-12-12 东华大学 等离子体耦合离子液体促进污泥产短链脂肪酸的应用

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